CN102507512A - On-line in situ detecting method for infrared-ultraviolet double pulse laser induced breakdown spectroscopy - Google Patents
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Abstract
The invention discloses an on-line in situ detecting method for an infrared-ultraviolet double pulse laser induced breakdown spectroscopy, which at least comprises the following steps of: A. setting a pulse delay time according to the sample excitation characteristics to control the time interval of two lasers; B. firstly outputting laser from an infrared waveband laser, long-distance collecting, adjusting and focusing on a position to be detected, and ablating the sample to generate plasma; C. outputting laser from an ultraviolet waveband laser after a delay time, long-distance collecting, adjusting and focusing on the same position, and exciting the plasma to reinforce a spectrum signal; D. receiving the spectrum signal through a long-distance spectrum collecting device, coupling the spectrum signal in an optical fiber, transmitting the spectrum signal to a spectrograph, and obtaining the spectrum data information through an assorted software; E. collecting the spectrum data, and obtaining a detection ingredient analysis result by a calibration-free correction analysis method.
Description
Technical field
The present invention can satisfy the strict demand of online in situ detection, adaptable across a plurality of technical fields such as analysis, detection, metering and diagnosis, is specifically related to a kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method.
Background technology
Online in situ detection technology is the new important component part of modern detecting; Can detect the performance of material in labour equipment fast, conveniently, effectively; Finding the damage of existing structure and fragile part, is the effective means of preventing accident and taking place and guaranteeing equipment operation safety.The technological difficulties of in situ detection mainly show as: detect on the one hand the field condition harshness, can't with ideal conditions analogy such as laboratory; Structure to be detected on the other hand or material etc. are in confined state, allow the time and the space of detection limited.Compare with the detection of offing normal, online in situ detection requires higher, and difficulty is bigger.
In situ detection generally comprises contents such as defect detection, fault diagnosis, condition monitoring and measured performance parameter; Wherein defect detection and measured performance parameter are used the most extensive; Both all are to be prerequisite to obtain sample composition information; Its result directly influences its detectivity and mensuration level, thereby it is most important accurately to measure the composition information of detected sample.
Traditional composition detection technology mainly contains X-ray fluorescence method, atomic absorption spectrum (AAS) method, inductively coupled plasma atomic emission (ICP-AES) method and inductively coupled plasma emission mass spectroscopy (ICP-MS) method.Wherein X-ray fluorescence method can be realized fast detecting, but its sensitivity is lower; Though and AAS method and ICP-AES method accuracy of detection are high, good stability, both all need the sample pretreatment process, are difficult to guarantee the not contaminated or loss of sample to be checked; And the ICP-MS method can remedy above-mentioned deficiency, but since checkout equipment cost an arm and a leg, bulky, testing process is consuming time longer, is difficult to satisfy the room and time requirement of in situ detection, can't realize widely applying.
LIBS technology (Laser Induced Breakdown Spectroscopy); Be called for short LIBS; As a kind of in real time, original position, continuous, contactless novel detection technique remedied the deficiency of above detection method, can satisfy the technical need of online in situ detection.This technology need not loaded down with trivial details sample pretreatment process; Solid (conductor or nonconductor), liquid or gaseous sample dimensional requirement to various forms are all not strict, and the sample consumption is extremely low, can carry out measuring simultaneously fast of multielement; Wide accommodation is convenient to remote control.
With the traditional detection compared with techniques, the LIBS technology has incomparable technical advantage for online in situ detection, but because the sensitivity of monopulse LIBS analysis of technology is not high, thereby restricted its application in the trace element detection range.LIBS is based on high power laser light and matter interaction, produces the transient state plasma, and the emission spectrum of article on plasma body (the continuous background spectra and the characteristic spectrum of element to be measured) is studied, thereby realizes qualitative analysis and quantitative test to sample composition.Plasma temperature that monopulse LIBS excites and density are all lower, and the intensity of emission spectra of formation is limited, thereby sensitivity for analysis is relatively low, and detection limit is higher relatively.
Summary of the invention
Deficiency in view of the traditional detection technology; A kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method that the present invention is based on the DP-LIBS technological invention; This detection method sample consumption is low to moderate about 0.1ug-0.1mg; The in-situ micro area spatial resolution can reach 1-100um, and its sensitivity for analysis exceeds the 1-2 one magnitude than monopulse LIBS technology.
A kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method provided by the invention may further comprise the steps:
Steps A. according to the exciting characteristic of detected sample, set the time delay of pulse delay controller, in order to control the time interval of two laser; Form the initial stage at plasma, atom gets into plasma from detected sample and needs several microseconds until evaporation fully, because the evaporation energy of different plant species element is different with the ablation amount, thereby the spectral line of element reaches the maximum emission intensity required time and also is not quite similar.
Step B. infrared band laser device is exported the ps pulsed laser and ns pulsed laser of infrared band earlier under the pulse delay controller triggers, via the long-range regulating device that converges of light beam, focus on sample surfaces position to be detected, and ablation sample position to be detected is to produce plasma.
Step C. ultraviolet band laser device is under the pulse delay controller triggers; The ps pulsed laser and ns pulsed laser of output ultraviolet band after one period time delay at interval; Via the long-range regulating device that converges of light beam, focus on the sample surfaces same position, activated plasma enhanced spectrum signal; The selection of two ps pulsed laser and ns pulsed laser wavelength, frequency and the intensity of step B and step C; Mainly the exciting characteristic by detected sample determines; To the different plant species element, can be in testing process online adjustment optical maser wavelength, frequency and intensity, to reach optimal detection condition.
The enhanced spectrum signal receives via spectrum long range acquisition device among the step D. step C, is coupled into optical fiber, transfers to spectrometer, through the sub computers program, can obtain all band spectroscopic data information.
Step e. according to gathering all band spectroscopic data information that obtains, utilize the physical parameter of plasma and freely calibrate the correction analysis method to draw detection constituent analysis conclusion.
The concrete steps of said step e are:
E1. according to gathering all band spectroscopic data information that obtains; Draw the measured line integral intensity
of the transition of a certain atomic species s between two different energy level Ek and Ei, be expressed as:
Wherein,
Be transition wavelength; Concentration for the emission atomic species;
Be the probability that jumps to particular spectral lines; Be k degeneracy of energy level degree;
Be Boltzmann constant;
Be plasma temperature; F is a constant, and is relevant with the efficient of light collecting device, what relation the pairing constant F of the light collecting device of different efficient is different (to have?), with Wavelength-independent, in testing process, remain unchanged;
BeThe partition function of emission species s is expressed as:
2. pairs of equations of step e (1) are taken the logarithm, and make following hypothesis:
?,，
?，
（3）
Obtain linear equation
about parameter y and x;
Step e 3. is according to
and known spectra parameter
and
in the spectra database that record; Can draw the straight line of y about x; Obtain slope m and intercept
; Can get through slope,
;
The concentration normalization of 4. pairs of all species compositions of step e can draw F, promptly
The concentration of species composition can calculate through formula
, can obtain detected sample constituent analysis result.
A kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method provided by the invention can be treated the sample article and realize that spot sampling detects, and accomplishes the accurate detection of original position analysis, real-time analysis and trace element.
The present invention adopts dipulse LIBS technology; Utilize the first bundle laser pulses irradiate sample surfaces to produce plasma; The second bundle laser pulses irradiate plasma is launched with enhanced line after a while; Realized distribution optimization, more can realize flexible optimization laser parameter (like energy, time etc.) if use two laser instruments to export two bundle laser respectively to two stages of material ablation and excitation of plasma.
In sum; A kind of infrared and ultraviolet double-pulse laser induced breakdown of the present invention spectrum on line in-situ detection method can effectively strengthen the spectral radiance of laser plasma, and prolong the relaxation time of radiation; Improve the sensitivity of spectral detection; Realization is treated sample article spot sampling and is detected, and realizes the accurate detection of original position analysis, real-time analysis and the trace element of sample, adaptable across a plurality of technical fields such as analysis, detection, metering and diagnosis.
Description of drawings
Fig. 1 is the structural representation of detection method detection device thereof of the present invention.
Fig. 2 is among Fig. 1, the long-range partial enlarged drawing that converges regulating device of light beam.
Fig. 3 is among Fig. 1, the partial enlarged drawing of optical radiation gathering-device.
Fig. 4 is the process flow diagram of detection method according to the invention.
Reference numeral and explanation: 1. infrared band laser device (is example with 1064nm Nd:YAG ps pulsed laser and ns pulsed laser device); 2. ultraviolet band laser device (is example with 193nm ArF quasi-molecule ps pulsed laser and ns pulsed laser device); 3. pulse delay controller; 4. the long-range regulating device that converges of first light beam; 5. the long-range regulating device that converges of second light beam; 6. the long-range receiving trap of spectrum; 7. seven passage high resolution micro optical fiber; 8. all band induced with laser attenuate light spectrometer; 9. computing machine; 10. condenser lens; 11. special catoptron; 12. first lens; 13. second lens; 14. the 3rd lens.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The pick-up unit structure that the inventive method adopted is: infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in situ detection device, core component comprise infrared band laser device (is example with 1064nm Nd:YAG ps pulsed laser and ns pulsed laser device), ultraviolet band laser device (is example with 193nm ArF quasi-molecule ps pulsed laser and ns pulsed laser device), pulse delay controller, long-range regulating device, the long-range receiving trap of spectrum, seven passage high resolution micro optical fiber, all band induced with laser attenuate light spectrometer and the computing machine etc. of converging of light beam.
The long-range regulating device that converges of said light beam is made up of condenser lens and special catoptron; Can realize that not only laser far-distance focuses on; Prolong and detect distance; And can realize freely selecting of detection angles and detection faces, thus overcome special-shaped device and detect the narrow and small constraint in space, realize that spot sampling detects.
The long-range receiving trap of said spectrum inside forms telescopic system by one group of lens, in the receiving spectrum signal process, guarantees that as far as possible the focus of telescopic system overlaps with the position of laser focusing in sample, in the hope of receiving more emission spectrum, improves signal to noise ratio (S/N ratio).
Because the pick-up unit principle of work that the present invention adopted is based on the DP-LIBS technology, it requires to detect the elemental composition that line strength characterized in all band spectroscopic data that is obtained and must be consistent with the elemental composition on actual sample surface.In theory, compare, can meet the demands through the alignment light spectrometer and with the spectral intensity signal of standard sources.But all band spectroscopic data not only depends on the geometric distributions of laser parameter, plasma in the actual detected process, also receives the influence (composition of sample, surface condition, thermodynamic property are referred to as matrix effect) of matrix effect.
Freely calibrate correction analysis method (calibration-free) based on following three reasonable assumptions:
A. the element composition that each element is formed and sample is ablated preceding in the plasma is identical;
B. in the time and space observation gate of reality, plasma is in hot plasma and is in the heat power balance;
C. transmitting illuminant is enough little.
Can remedy above-mentioned deficiency, overcome the influence of matrix effect, satisfy the strict demand of detection technique.
According to above-mentioned hypothesis; The transition measured line integral intensity of a certain atomic species s between two different energy level Ek and Ei can be expressed as in
(1) formula
,
，
?， （3）
Can about the linear equation
of parameter y and x according to
and the known spectra parameter
in the spectra database that record,
and; Can draw the straight line (Boltzmann curve) of y about x; Obtain slope m and intercept, can get (
) through slope.Concentration normalization to all species compositions can draw F, i.e.
and the concentration
of species composition can be passed through formula
Calculate, can obtain detected sample constituent analysis result.
Embodiment: extremely shown in Figure 3 like Fig. 1 is the structure of detection method detection device thereof according to the invention.Core component comprises infrared band laser device 1 (is example with 1064nm Nd:YAG ps pulsed laser and ns pulsed laser device); Ultraviolet band laser device 2 (is example with 193nm ArF quasi-molecule ps pulsed laser and ns pulsed laser device); Pulse delay controller 3; The long-range regulating device 4 that converges of first light beam; The long-range regulating device 5 that converges of second light beam; The long-range receiving trap 6 of spectrum; Seven passage high resolution micro optical fiber 7; All band induced with laser attenuate light spectrometer 8; With computing machine 9 etc.
Be illustrated in figure 4 as the process flow diagram of a kind of infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method according to the invention, comprising following steps:
The first step, according to the exciting characteristic of detected sample, set the time delay of pulse delay controller 3, in order to control the time interval of two laser.
Second step, infrared band laser device 1 (is example with 1064nm Nd:YAG ps pulsed laser and ns pulsed laser device); The ps pulsed laser and ns pulsed laser of first output high-power density under pulse delay controller 3 triggers; Via the long-range regulating device 4 that converges of first light beam; Focus on sample surfaces position to be detected, ablation sample position to be detected is to produce plasma.
The 3rd step, ultraviolet band laser device 2 (is example with 193nm ArF quasi-molecule ps pulsed laser and ns pulsed laser device); Under pulse delay controller 3 triggers; The ps pulsed laser and ns pulsed laser of output high-power density after one period time delay at interval; Via the long-range regulating device 5 that converges of second light beam, focus on the sample surfaces same position, activated plasma enhanced spectrum signal.
The 4th step, spectral signal receive via spectrum long range acquisition device 6, are coupled into optical fiber 7, transfer to spectrometer 8, through software kit, can obtain spectroscopic data information.
The 5th step, according to all band spectroscopic data information that gather to obtain; The physical parameter of line strength and plasma such as the energy of atomic transition, the mathematical relation between the plasma temperature are set up Quantitative Analysis Model, utilize and freely calibrate correction analysis method (calibration-free) and can draw detection constituent analysis conclusion.
Definite preferred embodiment that all belongs to of above-mentioned concrete detection method and optical maser wavelength; Can not limit claim of the present invention; Other any change or other equivalent substitute modes that does not deviate from the technical scheme of invention and made is included in protection scope of the present invention.
Claims (2)
1. infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method may further comprise the steps:
Steps A. according to the exciting characteristic of detected sample, set the time delay of pulse delay controller, in order to control the time interval of two laser;
Step B. infrared band laser device is exported the ps pulsed laser and ns pulsed laser of infrared band earlier under the pulse delay controller triggers, via the long-range regulating device that converges of light beam, focus on sample surfaces position to be detected, and ablation sample position to be detected is to produce plasma;
Step C. ultraviolet band laser device is under the pulse delay controller triggers; The ps pulsed laser and ns pulsed laser of output ultraviolet band after one period time delay at interval; Via the long-range regulating device that converges of light beam, focus on the sample surfaces same position, activated plasma enhanced spectrum signal;
The enhanced spectrum signal receives via spectrum long range acquisition device among the step D. step C, is coupled into optical fiber, transfers to spectrometer, through the sub computers program, can obtain all band spectroscopic data information;
Step e. according to gathering all band spectroscopic data information that obtains, utilize the physical parameter of plasma and freely calibrate the correction analysis method to draw detection constituent analysis conclusion.
2. infrared and ultraviolet double-pulse laser induced breakdown spectrum on line in-situ detection method according to claim 1 is characterized in that the concrete steps of said step e are:
E1. according to gathering all band spectroscopic data information that obtains; Draw the measured line integral intensity
of the transition of a certain atomic species s between two different energy level Ek and Ei, be expressed as:
Wherein,
Be transition wavelength;
Concentration for the emission atomic species;
Be the probability that jumps to particular spectral lines;
Be k degeneracy of energy level degree;
Be Boltzmann constant;
Be plasma temperature; F is a constant, and is relevant with the efficient of light collecting device, with Wavelength-independent, in testing process, remains unchanged;
BeThe partition function of emission species s is expressed as:
2. pairs of equations of step e (1) are taken the logarithm, and make following hypothesis:
Obtain linear equation
about parameter y and x;
Step e 3. is according to
and the known spectra parameter
in the spectra database,
and
that record; Can draw the straight line of y about x; Obtain slope m and intercept
; Can get through slope,
;
The concentration normalization of 4. pairs of all species compositions of step e can draw F, promptly
The concentration of species composition
can calculate through formula, can obtain detected sample constituent analysis result.
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Cited By (15)
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| CN102788772A (en) * | 2012-07-13 | 2012-11-21 | 国电燃料有限公司 | Method for measuring content of powdery substantial elements based on dual pluses |
| CN103196772A (en) * | 2013-04-03 | 2013-07-10 | 大连理工大学 | Method for performing on-line measurement on stoichiometric ratio and component mass of PLD (Pulsed Laser Deposition) membrane |
| CN103398988A (en) * | 2013-08-08 | 2013-11-20 | 南昌航空大学 | LIBS metal element quantification method based on different element multi-ion-state comparison and correction |
| WO2015007041A1 (en) * | 2013-07-15 | 2015-01-22 | 中国科学院沈阳自动化研究所 | In-situ on-line detection device and method for long-distance metallurgical liquid metal component |
| WO2015030619A1 (en) * | 2013-08-28 | 2015-03-05 | Institutul National De Cercetare - Dezvoltare Pentru Fizica Laserilor, Plasmei Si Radiaţiei | System and method for testing components, circuits and complex systems using synchronized and pulsed fluxes consisting of laser accelerated particles |
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| CN104931462A (en) * | 2014-03-17 | 2015-09-23 | 以恒科技(北京)有限公司 | Mixed light source focusing enhancing plasma detection system |
| CN105203526A (en) * | 2015-09-22 | 2015-12-30 | 中国科学院上海技术物理研究所 | Calibration-free remote quantitative laser-induced breakdown spectroscopy analysis method |
| CN105556291A (en) * | 2013-05-30 | 2016-05-04 | 激光测距光谱有限公司 | Method of laser-induced breakdown spectroscopy in air |
| CN106442431A (en) * | 2016-08-31 | 2017-02-22 | 广州博谱能源科技有限公司 | Correction method for improving repeatability of LIBS (Laser-Induced Breakdown Spectroscopy) technique measured sample |
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| CN102788772A (en) * | 2012-07-13 | 2012-11-21 | 国电燃料有限公司 | Method for measuring content of powdery substantial elements based on dual pluses |
| CN103196772A (en) * | 2013-04-03 | 2013-07-10 | 大连理工大学 | Method for performing on-line measurement on stoichiometric ratio and component mass of PLD (Pulsed Laser Deposition) membrane |
| CN105556291A (en) * | 2013-05-30 | 2016-05-04 | 激光测距光谱有限公司 | Method of laser-induced breakdown spectroscopy in air |
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